反应详情

温度

120 °C

(+/−)-(trans)-4-(4-Methyl-3-oxo-cyclohexyl)benzonitrile (0.55 g, 2.58 mmol) is added to toluene (10.0 mL) and tert-butoxybis(dimtheylamino)methane (0.67 mL, 3.22 mmols) and stirred at 120° C. for 16 hours. The mixture is cooled to room temperature and concentrated in vacuo. The residue is added to MeOH (10.0 mL) and hydrazine (0.07 mL, 2.32 mmol) and stirred at 80° C. for 1.0 hour. The mixture is cooled to room temperature and concentrated in vacuo. The residue is purified by silica gel chromatography (35%-55% EtOAc/hexanes) to give (+/−)-(trans)-4-[7-methyl-4,5,6,7-tetrahydro-2H-indazol-4-yl]benzonitrile (0.18 g, 29%).

1. temperatureThe mixture is cooled to room temperature
2. concentrationconcentrated in vacuo
3. stirringstirred at 80° C. for 1.0 hour
4. temperatureThe mixture is cooled to room temperature
5. concentrationconcentrated in vacuo
6. customThe residue is purified by silica gel chromatography (35%-55% EtOAc/hexanes)